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CN114394839B - 一种氮化碳基复合陶瓷刀具材料、其制备方法与切削刀具 - Google Patents

一种氮化碳基复合陶瓷刀具材料、其制备方法与切削刀具 Download PDF

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CN114394839B
CN114394839B CN202210026265.3A CN202210026265A CN114394839B CN 114394839 B CN114394839 B CN 114394839B CN 202210026265 A CN202210026265 A CN 202210026265A CN 114394839 B CN114394839 B CN 114394839B
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carbon nitride
powder
composite ceramic
molybdenum
nickel
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CN114394839A (zh
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黄传真
张岩
刘含莲
史振宇
姚鹏
王真
徐龙华
黄水泉
王军
朱洪涛
邹斌
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Shandong University
Yanshan University
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Yanshan University
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Abstract

本发明涉及新材料技术领域，尤其涉及一种氮化碳复合陶瓷刀具材料、其制备方法与切削刀具，其原料包括氮化碳、碳氮化钛、钼、镍和钴，以氮化碳作为基体相，碳氮化钛作为增强相添加到氮化碳基复合陶瓷材料中，配以钼、镍和钴作为合适的烧结助剂，通过真空热压烧结工艺制备出致密的复合刀具材料。制备的氮化碳基复合陶瓷刀具材料具有低成本、高硬度、高抗弯强度和高断裂韧度等优势，是促进氮化碳材料的创新、发展、推广应用的重要途径。

Description

一种氮化碳基复合陶瓷刀具材料、其制备方法与切削刀具
技术领域
本发明涉及新材料技术领域，尤其涉及一种氮化碳基复合陶瓷刀具材料、其制备方法与切削刀具。
背景技术
公开该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。
据发明人研究了解，氮化碳目前在刀具领域的应用只是作为涂层。氮化碳涂层刀具表面硬度高，使用寿命显著延长，适于高速精加工，但是当涂层破损后刀具切削性能明显下降。氮化碳具有较高的熔点、高硬度、优异的化学稳定性，但其作为基体相烧结性能较差。
发明内容
针对现有技术中存在的问题，本发明提供氮化碳复合陶瓷刀具材料、其制备方法与切削刀具。制备的氮化碳基复合陶瓷刀具材料具有低成本、高硬度、高抗弯强度和高断裂韧度等优势，是促进氮化碳材料的创新、发展、推广应用的重要途径。
为解决以上技术问题，本发明的以下一个或多个实施例提供了如下技术方案：
第一方面，本发明提供一种氮化碳基复合陶瓷刀具材料，其原料包括氮化碳、碳氮化钛、钼、镍和钴，氮化碳、碳氮化钛、钼、镍和钴的重量比(％)为40-70：20-45：2-8：2-8：2-8。
以氮化碳作为基体相，需要添加增强相和烧结助剂，才能保证氮化碳基复合陶瓷刀具材料的力学性能，本发明经过研究表明，当碳氮化钛作为增强相时烧结助剂的添加种类对于氮化碳基复合陶瓷刀具材料的力学性能影响较大，此时，以钼、镍和钴作为烧结助剂时，能够保证氮化碳基复合陶瓷刀具材料的力学性能。
第二方面，本发明提供一种上述氮化碳基复合陶瓷刀具材料的制备方法，包括如下步骤：
分别对氮化碳、碳氮化钛、钼、镍和钴进行单独球磨；
将球磨后的原料粉末按设定比例混合球磨、干燥，得到混合物料；
将混合物料进行真空热压烧结，得到氮化碳基复合陶瓷刀具材料。
本发明以氮化碳作为基体相，碳氮化钛作为增强相添加到氮化碳基复合陶瓷材料中，配以钼、镍和钴作为烧结助剂，通过真空热压烧结工艺制备出致密的复合刀具材料，从而提高氮化碳基复合陶瓷刀具材料的力学性能。
第三方面，本发明提供一种切削刀具，由上述氮化碳基复合陶瓷刀具材料制备而成。
与现有技术相比，本发明的以上一个或多个技术方案取得了以下有益效果：
本发明所使用的设备简单且安全性好，制备工艺稳定，操作处理简单，生产效率高。该工艺通过以氮化碳为复合陶瓷材料的基体相，添加增强相，并优化材料组分配比、烧结温度、保温时间等参数，制备出了一种新型氮化碳基复合陶瓷刀具材料，是氮化碳在陶瓷刀具材料领域的全新应用。
氮化碳基复合陶瓷刀具材料具有低成本、高硬度、高抗弯强度和高断裂韧度等优势，是促进氮化碳材料的创新、发展、推广应用的重要途径。
附图说明
图1为本发明实施例1制备的氮化碳基复合陶瓷刀具材料的SEM图。
具体实施方式
应该指出，以下详细说明都是示例性的，旨在对本发明提供进一步的说明。除非另有指明，本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是，这里所使用的术语仅是为了描述具体实施方式，而非意图限制根据本发明的示例性实施方式。如在这里所使用的，除非上下文另外明确指出，否则单数形式也意图包括复数形式，此外，还应当理解的是，当在本说明书中使用术语“包含”和/或“包括”时，其指明存在特征、步骤、操作、器件、组件和/或它们的组合。
本发明的一种典型实施方式，提供了一种氮化碳基复合陶瓷刀具材料，其原料包括氮化碳、碳氮化钛、钼、镍和钴，氮化碳、碳氮化钛、钼、镍和钴的重量比(％)为40-70：20-45：2-8：2-8：2-8。
本发明中，氮化碳作为基体相，碳氮化钛为增强相，钼、镍和钴为金属相烧结助剂。研究表明，以上述原料获得的氮化碳基复合陶瓷刀具材料的力学性能具有更优的力学性能，从而能够使氮化碳作为基体相用于制备陶瓷刀具。
在一些实施例中，氮化碳、碳氮化钛、钼、镍、钴的重量比(％)为48-63：25-40：3-5：3-5：3-5。
在一些实施例中，氮化碳的粒径为1～5μm。
在一些实施例中，碳氮化钛的粒径为0.5～1.5μm。
在一些实施例中，钼的粒径为0.5～1.5μm。
在一些实施例中，镍的粒径为0.5～1.5μm。
在一些实施例中，钴的粒径为0.5～1.5μm。
本发明的第二种实施方式，提供了一种上述氮化碳基复合陶瓷刀具材料的制备方法，包括如下步骤：
分别对氮化碳、碳氮化钛、钼、镍和钴进行单独球磨；
将球磨后的原料粉末按设定比例混合球磨、干燥，得到混合物料；
将混合物料进行真空热压烧结，得到氮化碳基复合陶瓷刀具材料。
在一些实施例中，氮化碳、碳氮化钛、钼、镍和钴分别进行单独球磨的球磨介质为无水乙醇。加入无水乙醇能使物料具有一定的流动性和粘性，起到分散剂的作用；而且球磨后的物料在烘干的过程中，无水乙醇会完全挥发，没有残余。
进一步的，氮化碳、碳氮化钛、钼、镍和钴原料球磨的时间为60-72h。
进一步的，经过球磨后的原料粉末的干燥温度为100-120℃。
更进一步的，经过干燥后的原料粉末过100目筛。
进一步的，混合球磨的介质为无水乙醇。以便于使各相材料混合更加均匀。
本发明中所述的真空热压烧结是指，在真空条件下，先进行模压成型，然后进行烧结的过程。在一些实施例中，真空热压烧结的工艺条件为：以40-60℃/min的升温速率从15-25℃开始加热到950-1050℃，同时加压至7.5-8.5MPa；然后以15-35℃/min的升温速率加热到1450-1600℃，同时压力均匀加至28-35MPa；保温保压时间为15-85min。以15-35℃/min的升温速率加热到的温度可以为1445-1455℃、1495-1505℃、1545-1555℃或1595-1600℃。升温至1450-1600℃加压后的保温保压时间可以为15-25min、35-45min、55-65min或75-85min。
进一步的，热压烧结的工艺条件为：以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1450℃、1500℃、1550℃或1600℃，同时压力均匀加至32MPa；保温保压时间为20min、40min、60min或80min。
在一些实施例中，烧结完毕后，将烧结材料随炉冷却，即得氮化碳基复合陶瓷刀具材料。
本发明的第三种实施方式，提供了一种切削刀具，由上述氮化碳基复合陶瓷刀具材料制备而成。
实施例1：
1)用无水乙醇作为介质，分别对氮化碳、碳氮化钛、钼、镍和钴原料粉末进行单独球磨，球磨过程是在滚筒式球磨机上进行的，其中，将氮化碳粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为5μm的粉末；碳氮化钛粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钼粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；镍粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钴粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末，之后都经过真空干燥，干燥温度为120℃，干燥后过100目筛，过筛后的粉体封装以备用；
2)按实施例参数附表，将63％重量比粒径为5μm的氮化碳粉末、25％重量比粒径为0.5μm的碳氮化钛粉末、4％重量比粒径为0.5μm的钼粉末、4％重量比粒径为0.5μm的镍粉末、4％重量比粒径为0.5μm的钴粉末，倒入混料桶中，加入无水乙醇作为介质，在球磨机上球磨48h，以使各相材料混合均匀，再经过120℃真空干燥、过100目筛，得到分散良好的复合陶瓷材料粉末料，封装以备用；
3)将混合好的复合陶瓷材料粉末装入石墨模具，放入真空热压烧结炉，在真空环境中，采用均匀加压的热压烧结工艺；以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1600℃，同时压力均匀加至32MPa；保温保压时间为60min；之后随炉冷却至20℃，即得所述氮化碳基复合陶瓷刀具材料，如图1所示，可见该刀具材料的组织致密，晶粒细小、均匀。
本实施例的试验参数，如表1所示。
表1
Figure BDA0003464794520000061
实施例2：
1)用无水乙醇作为介质，分别对氮化碳、碳氮化钛、钼、镍和钴原料粉末进行单独球磨，球磨过程是在滚筒式球磨机上进行的，其中，将氮化碳粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为5μm的粉末；碳氮化钛粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钼粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；镍粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钴粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末，之后都经过真空干燥，干燥温度为120℃，干燥后过100目筛，过筛后的粉体封装以备用；
2)按实施例参数附表，将58％重量比粒径为5μm的氮化碳粉末、30％重量比粒径为0.5μm的碳氮化钛粉末、4％重量比粒径为0.5μm的钼粉末、4％重量比粒径为0.5μm的镍粉末、4％重量比粒径为0.5μm的钴粉末，倒入混料桶中，加入无水乙醇作为介质，在球磨机上球磨48h，以使各相材料混合均匀，再经过120℃真空干燥、过100目筛，得到分散良好的复合陶瓷材料粉末料，封装以备用；
3)将混合好的复合陶瓷材料粉末装入石墨模具，放入真空热压烧结炉，在真空环境中，采用均匀加压的热压烧结工艺；以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1600℃，同时压力均匀加至32MPa；保温保压时间为60min；之后随炉冷却至20℃，即得所述氮化碳基复合陶瓷刀具材料。
本实施例的试验参数，如表1所示。
实施例3：
1)用无水乙醇作为介质，分别对氮化碳、碳氮化钛、钼、镍和钴原料粉末进行单独球磨，球磨过程是在滚筒式球磨机上进行的，其中，将氮化碳粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为5μm的粉末；碳氮化钛粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钼粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；镍粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钴粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末，之后都经过真空干燥，干燥温度为120℃，干燥后过100目筛，过筛后的粉体封装以备用；
2)按实施例参数附表，将53％重量比粒径为5μm的氮化碳粉末、35％重量比粒径为0.5μm的碳氮化钛粉末、4％重量比粒径为0.5μm的钼粉末、4％重量比粒径为0.5μm的镍粉末、4％重量比粒径为0.5μm的钴粉末，倒入混料桶中，加入无水乙醇作为介质，在球磨机上球磨48h，以使各相材料混合均匀，再经过120℃真空干燥、过100目筛，得到分散良好的复合陶瓷材料粉末料，封装以备用；
3)将混合好的复合陶瓷材料粉末装入石墨模具，放入真空热压烧结炉，在真空环境中，采用均匀加压的热压烧结工艺；以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1600℃，同时压力均匀加至32MPa；保温保压时间为60min；之后炉内随炉冷却至20℃，即得所述氮化碳基复合陶瓷刀具材料。
本实施例的试验参数，如表1所示。
实施例4：
1)用无水乙醇作为介质，分别对氮化碳、碳氮化钛、钼、镍和钴原料粉末进行单独球磨，球磨过程是在滚筒式球磨机上进行的，其中，将氮化碳粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为5μm的粉末；碳氮化钛粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钼粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；镍粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末；钴粉末球磨72h以分散较大的团聚颗粒，获得均匀的粒径为0.5μm的粉末，之后都经过真空干燥，干燥温度为120℃，干燥后过100目筛，过筛后的粉体封装以备用；
2)按实施例参数附表，将48％重量比粒径为5μm的氮化碳粉末、40％重量比粒径为0.5μm的碳氮化钛粉末、4％重量比粒径为0.5μm的钼粉末、4％重量比粒径为0.5μm的镍粉末、4％重量比粒径为0.5μm的钴粉末，倒入混料桶中，加入无水乙醇作为介质，在球磨机上球磨48h，以使各相材料混合均匀，再经过120℃真空干燥、过100目筛，得到分散良好的复合陶瓷材料粉末料，封装以备用；
3)将混合好的复合陶瓷材料粉末装入石墨模具，放入真空热压烧结炉，在真空环境中，采用均匀加压的热压烧结工艺；以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1600℃，同时压力均匀加至32MPa；保温保压时间为60min；之后随炉冷却至20℃，即得所述氮化碳基复合陶瓷刀具材料。
本实施例的试验参数，如表1所示。
对比例1
与实施例1的区别点在于：省略碳氮化钛，其它与实施例1的相同。
对比例2
与实施例1的区别点在于：省略钼，其他与实施例1的相同。
对比例3
与实施例1的区别点在于：省略镍，其他与实施例1的相同。
对比例4
与实施例1的区别点在于：省略钴，其他与实施例1的相同。
实施例1-4、对比例1-4中制备氮化碳基复合陶瓷刀具材料的力学性能如表2所示，可见实施例的维氏硬度、抗弯强度、断裂韧度均有较大提高。
表2
Figure BDA0003464794520000091
Figure BDA0003464794520000101
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种氮化碳基复合陶瓷刀具材料的制备方法，其特征在于：包括如下步骤：
分别对氮化碳、碳氮化钛、钼、镍和钴进行单独球磨；
将球磨后的原料粉末按设定比例混合球磨、干燥，得到混合物料；氮化碳、碳氮化钛、钼、镍和钴的重量比为40-70：20-45：2-8：2-8：2-8；
将混合物料进行真空热压烧结，得到氮化碳基复合陶瓷刀具材料；
真空热压烧结的工艺条件为：以40-60℃/min的升温速率从15-25℃开始加热到950-1050℃，同时加压至7.5-8.5MPa；然后以15-35℃/min的升温速率加热到1450-1600℃，同时压力均匀加至28-35MPa；保温保压时间为15-85min。
2.根据权利要求1所述的制备方法，其特征在于：氮化碳、碳氮化钛、钼、镍和钴的重量比为48-63：25-40：3-5：3-5：3-5。
3.根据权利要求1所述的制备方法，其特征在于：氮化碳的粒径为1~5μm；
或，碳氮化钛的粒径为0.5~1.5μm；
或，钼的粒径为0.5~1.5μm；
或，镍化钇的粒径为0.5~1.5μm；
或，钴化钇的粒径为0.5~1.5μm。
4.根据权利要求1所述的制备方法，其特征在于：氮化碳、碳氮化钛、钼、镍和钴原料粉末进行单独球磨的球磨介质为无水乙醇。
5.根据权利要求1所述的制备方法，其特征在于：氮化碳、碳氮化钛、钼、镍和钴原料单独球磨的时间分别为60-72h；
或，经过球磨后的原料粉末的干燥温度为100-120℃；
经过干燥后的原料粉末过100目筛。
6.根据权利要求1所述的制备方法，其特征在于：混合球磨的介质为无水乙醇。
7.根据权利要求1所述的制备方法，其特征在于：真空热压烧结的工艺条件为：以50℃/min的升温速率从20℃开始加热到1000℃，同时加压至8MPa；然后以30℃/min的升温速率加热到1450℃、1500℃、1550℃或1600℃，同时压力均匀加至32MPa；保温保压时间为20min、40min、60min或80min。
8.根据权利要求1所述的制备方法，其特征在于：烧结完毕后，将烧结材料随炉冷却，即得氮化碳基复合陶瓷刀具材料。
9.一种切削刀具，其特征在于：由权利要求1-8任一所述氮化碳基复合陶瓷刀具材料的制备方法制备而成。
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